WO2001098751A1 - Method for determining surface tension of a comminuted solid - Google Patents
Method for determining surface tension of a comminuted solid Download PDFInfo
- Publication number
- WO2001098751A1 WO2001098751A1 PCT/FR2001/001906 FR0101906W WO0198751A1 WO 2001098751 A1 WO2001098751 A1 WO 2001098751A1 FR 0101906 W FR0101906 W FR 0101906W WO 0198751 A1 WO0198751 A1 WO 0198751A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- liquid
- tube
- equation
- solid
- mass
- Prior art date
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/02—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by absorbing or adsorbing components of a material and determining change of weight of the adsorbent, e.g. determining moisture content
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
- G01N13/02—Investigating surface tension of liquids
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/088—Investigating volume, surface area, size or distribution of pores; Porosimetry
Definitions
- the present invention relates to a method for determining the surface energy of a finely divided solid, so as to better define its surface characteristics and properties.
- this process uses the combination of different experimental measurements with mathematical equations.
- the various chemical industries which use finely divided solids (also called powder) to prepare compositions, regularly face problems when dispersing the powder in a liquid, or when drying the powder which very easily tends to to agglomerate, or quite the contrary after being compressed, disintegrates with difficulty or then too easily.
- the kinetics of capillary rise is obtained by following the variation in mass of the tube filled with powder, over time.
- the subject of the invention is therefore a method for determining the surface energy ⁇ s of a finely divided solid from various experimental measurements and different mathematical equations consisting of:
- - A is the specific area of the finely divided solid (m 2 / m 3 )
- - ⁇ P is the pressure variation applied to the tube, to stop, in a third phase, the application of the first counter pressure so as to allow the liquid to rise freely in the tube until the divided solid is completely submerged in the liquid present in the tube, and to regularly measure the variation in the mass of liquid remaining, after the liquid has risen in the tube, as a function of time, to then deduce after mathematical calculation the total mass of the liquid mounted in the tube, and then obtain, after application of the mathematical equation (I), the slope 2, then the porosity ⁇ according to the following equation (III):
- - R is the internal radius of the tube
- - ⁇ P is the pressure variation applied to the tube
- - ⁇ is the viscosity of the liquid
- a second counter pressure kept constant for a period ranging from approximately 300 to 1000 seconds so as to calculate again the numerical value of the specific area A (m 2 / m 3 ) as defined in step 4.
- the invention has the advantage of determining the surface energy ⁇ s of a powder in a simple, rapid, reliable and perfectly reproducible manner, and with only one probe liquid.
- the subject of the invention is also a use of the method as defined above for determining the surface energy of finely divided solid entering into the chemical composition of solid-liquid dispersion, of paints, inks, adhesives, resins .
- a final object of the invention relates to the use of the method defined above for determining the surface energy of a finely divided, agglomerated solid.
- the porosity value ⁇ is easily accessible experimentally. Indeed, when the liquid soaks the entire tube partially filled with the powder having a height "h", the weight gain of the tube "m” gives directly, after mathematical calculation, the value of the tortuosity ⁇ .
- the divided solid is chosen from mineral solids which may be in the finely divided state, such as organic or mineral polymers of synthetic origin such as, for example, polytetrafluoroethylene (PTFE) or polyethylene, or also from polymers organic or minerals of natural origin such as talc, glass, flour of various cereals or among the bacterial walls.
- organic or mineral polymers of synthetic origin such as, for example, polytetrafluoroethylene (PTFE) or polyethylene
- PTFE polytetrafluoroethylene
- polyethylene polyethylene
- polymers organic or minerals of natural origin such as talc, glass, flour of various cereals or among the bacterial walls.
- the liquid can be chosen from alkanes such as pentane, hexane, heptane, octane, nonane, decane, cyclohexane, hexadecane, cis-decaline, 1 ' ⁇ -bromonaphthalene, diiodomethane, or among other organic compounds such as methanol, ethanol, methyl ethyl ketone, tetrahydrofuran (THF), ethylene glycol, glycerol, formamide, dimethyl sulfoxide, 1, 'water.
- alkanes such as pentane, hexane, heptane, octane, nonane, decane, cyclohexane, hexadecane, cis-decaline, 1 ' ⁇ -bromonaphthalene, diiodomethane, or among other organic compounds such as methanol, ethanol, methyl e
- the liquid can have an average density between 0.6 and 3.5 and an average viscosity between 0.1 and 1000 mPa.s.
- the first back pressure applied during the second step can be between 5 and 800 mbar.
- the vacuum applied during the fourth step can be between 5 and 200 mbar.
- the second back pressure applied during the fifth step can be between 5 and 200 mbar.
- the first and second steps can be repeated 3 or 4 times when the rise in the liquid is less than or equal to 10 mm.
- the permeable membrane used is preferably chosen from membranes of a cellulose nature conventionally made of cellulose acetate or of cellulose nitrate having cut-off thresholds of the order of 1 to 10 ⁇ m, or among the membranes composed of glass microfibers having similar cutoff thresholds.
- the vacuum of the fourth step and the second back pressure of the fifth step are preferably applied respectively for durations varying from 60 seconds to 600 seconds.
- FIG. 1 is a schematic sectional view of the various elements constituting the apparatus intended to take the experimental measurements during the implementation of the method of the invention
- figure 3 represents the different applications of back pressure and vacuum during the process according to example 1
- a glass reference tube 1 having an internal diameter of 8 mm, a section of 5.02610 "s m 2 , and a total height which can vary from 30 to 120 mm is hermetically sealed. on its lower part 1a by a membrane 2, permeable to liquid and constituted by a filter paper.
- the tube 1 is then filled to about 80% of its total height, with a finely divided solid 3 such as for example polytetrafluoroethylene (PTFE) or also with polyethylene.
- a finely divided solid 3 such as for example polytetrafluoroethylene (PTFE) or also with polyethylene.
- the solid can also consist of any chemical components of mineral or organic nature which can be put into a pulverulent state and which is insoluble in the probe liquid. The solid is packed mechanically and very carefully in the tube.
- the lower part 1a of the tube 1 is then immersed in a liquid 4 placed in a cup 5.
- the liquid 4 is for example hexane, and has a density p of 660 kg / m2 and a viscosity ⁇ of 3.10 "4 Pa .s.
- the cup 5 rests directly on a balance 6 having an accuracy ranging from 1/100 to 1/1000 g.
- the balance 6 is also connected to a computer data processing system (not shown).
- the liquid 4 rises freely by capillary action and in a known manner in the tube 1 through the permeable membrane 2 and the powder 3 up to 10 to 20% of its height of powder, so as to leave a portion of the powder not impregnated with the liquid 4.
- a first vertical back pressure P x directed from top to bottom is applied during the second step using d a syringe 7.
- the syringe 7 is filled with a gas, generally dry air or any other gas inert towards the liquid or the solid such as, for example, nitrogen, carbon dioxide, or more helium.
- the syringe 7 makes it possible to repel the liquid 4 partially mounted in the tube 1 in a regular and controlled manner.
- the syringe 7 makes it possible to apply an isostatic pressure P x due to the direct presence of the "pushing" gas on the probe liquid 4.
- the syringe 7 is actuated using a movable actuator 7a.
- the syringe 7 is connected to the tube 1 by means of a pressure sensor 8, itself connected to a solenoid valve 9 for bringing it to atmospheric pressure, and it is connected to a seal 10 directly on the upper part 1b of the tube .
- the back pressure P x is equal to 209 mbar and the height of liquid 4 in the tube is 30.9 mm.
Abstract
Description
Claims
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP01947523A EP1301768A1 (en) | 2000-06-20 | 2001-06-19 | Method for determining surface tension of a comminuted solid |
JP2002504463A JP2004503741A (en) | 2000-06-20 | 2001-06-19 | Method for measuring surface tension of pulverized solid |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR00/07878 | 2000-06-20 | ||
FR0007878A FR2810401B1 (en) | 2000-06-20 | 2000-06-20 | METHOD FOR DETERMINING THE SURFACE ENERGY OF A FINELY DIVIDED SOLID |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2001098751A1 true WO2001098751A1 (en) | 2001-12-27 |
Family
ID=8851461
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/FR2001/001906 WO2001098751A1 (en) | 2000-06-20 | 2001-06-19 | Method for determining surface tension of a comminuted solid |
Country Status (5)
Country | Link |
---|---|
US (1) | US20030164027A1 (en) |
EP (1) | EP1301768A1 (en) |
JP (1) | JP2004503741A (en) |
FR (1) | FR2810401B1 (en) |
WO (1) | WO2001098751A1 (en) |
Families Citing this family (13)
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---|---|---|---|---|
US7776604B2 (en) * | 2003-04-01 | 2010-08-17 | Cabot Corporation | Methods of selecting and developing a particulate material |
US7000457B2 (en) * | 2003-04-01 | 2006-02-21 | Cabot Corporation | Methods to control and/or predict rheological properties |
US7776602B2 (en) * | 2003-04-01 | 2010-08-17 | Cabot Corporation | Methods of providing product consistency |
US7776603B2 (en) * | 2003-04-01 | 2010-08-17 | Cabot Corporation | Methods of specifying or identifying particulate material |
US20040197924A1 (en) * | 2003-04-01 | 2004-10-07 | Murphy Lawrence J. | Liquid absorptometry method of providing product consistency |
US20050200056A1 (en) * | 2004-03-12 | 2005-09-15 | Heraeus Electro-Nite International N.V. | Apparatus and method for determining fluid depth |
US7246515B2 (en) * | 2005-03-15 | 2007-07-24 | Hewlett-Packard Development Company, L.P. | Filtration tester |
US7722713B2 (en) * | 2005-05-17 | 2010-05-25 | Cabot Corporation | Carbon blacks and polymers containing the same |
CN104359798B (en) * | 2014-10-10 | 2017-05-17 | 天津大学 | Multi-flux device capable of automatically measuring surface free energy parameters of powder/particles |
RU2653114C1 (en) * | 2017-02-02 | 2018-05-07 | Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский технологический университет "МИСиС" | Device for measurement of surface tension and metal viscosity factor |
US11080440B2 (en) | 2017-06-27 | 2021-08-03 | International Business Machines Corporation | Characterizing fluid flow at field conditions |
JP7079394B2 (en) * | 2018-02-21 | 2022-06-02 | 学校法人法政大学 | Contact angle measuring method and contact angle measuring device |
CN108872045A (en) * | 2018-08-06 | 2018-11-23 | 四川杰瑞泰克科技有限公司 | A kind of measurement method of the broken sample total porosity of shale |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE2116476A1 (en) * | 1971-04-03 | 1972-10-19 | Fraunhofer Ges Forschung | Method and device for measuring contact angles and heat of wetting between poorly wetting liquids and powders |
JPS6184546A (en) * | 1984-10-02 | 1986-04-30 | Sankyo Dengiyou Kk | Instrument for measuring wettability of powdery and granular material |
JPH01209339A (en) * | 1988-02-17 | 1989-08-23 | Sankyo Dengyo Co Ltd | Apparatus and method for measuring wetting of powdery granular material |
US5425265A (en) * | 1993-12-20 | 1995-06-20 | Jaisinghani; Rajan A. | Apparatus and method for measuring the capillary pressure distribution of porous materials |
DE19844595C1 (en) * | 1998-07-23 | 2000-01-05 | Fraunhofer Ges Forschung | Imbibition measurement arrangement for determining moistening characteristics of powders |
-
2000
- 2000-06-20 FR FR0007878A patent/FR2810401B1/en not_active Expired - Fee Related
-
2001
- 2001-06-19 US US10/311,992 patent/US20030164027A1/en not_active Abandoned
- 2001-06-19 WO PCT/FR2001/001906 patent/WO2001098751A1/en not_active Application Discontinuation
- 2001-06-19 JP JP2002504463A patent/JP2004503741A/en not_active Withdrawn
- 2001-06-19 EP EP01947523A patent/EP1301768A1/en not_active Withdrawn
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE2116476A1 (en) * | 1971-04-03 | 1972-10-19 | Fraunhofer Ges Forschung | Method and device for measuring contact angles and heat of wetting between poorly wetting liquids and powders |
JPS6184546A (en) * | 1984-10-02 | 1986-04-30 | Sankyo Dengiyou Kk | Instrument for measuring wettability of powdery and granular material |
JPH01209339A (en) * | 1988-02-17 | 1989-08-23 | Sankyo Dengyo Co Ltd | Apparatus and method for measuring wetting of powdery granular material |
US5425265A (en) * | 1993-12-20 | 1995-06-20 | Jaisinghani; Rajan A. | Apparatus and method for measuring the capillary pressure distribution of porous materials |
DE19844595C1 (en) * | 1998-07-23 | 2000-01-05 | Fraunhofer Ges Forschung | Imbibition measurement arrangement for determining moistening characteristics of powders |
Non-Patent Citations (7)
Title |
---|
BRUIL H G ET AL: "DETERMINATION OF CONTACT ANGLES OF AQUEOUS SURFACTANT SOLUTIONS ON POWDERS", COLLOID & POLYMER SCIENCE,DE,DARMSTADT, vol. 252, no. 1, January 1974 (1974-01-01), pages 32 - 38, XP002117218 * |
G.K.TAMPY ET AL.: "measurement of surface properties of coal ...", PREPRINTS OF PAPERS PRESENTED - AMERICAN CHEMICAL SOCIETY. DIVISION OF FUEL CHEMISTRY, vol. 32, no. 1, 1987, WASHINGTON, DC, US, pages 441 - 447, XP000989505, ISSN: 0569-3772 * |
PATENT ABSTRACTS OF JAPAN vol. 010, no. 256 (P - 493) 2 September 1986 (1986-09-02) * |
PATENT ABSTRACTS OF JAPAN vol. 013, no. 511 (P - 961) 16 November 1989 (1989-11-16) * |
SCHINDLER B ET AL: "Benetzungskinetik an Glaspulverschüttungen", CHEMIE. INGENIEUR. TECHNIK,DE,VERLAG CHEMIE GMBH. WEINHEIM, vol. 45, no. 9/10, May 1973 (1973-05-01), pages 583 - 586, XP002117217, ISSN: 0009-286X * |
SIEBOLD ET AL.: "effect of dynamic contact angle ...", COLLOIDS AND SURFACES, no. 161, 15 January 2000 (2000-01-15), pages 81 - 87, XP000987226 * |
SUBRAHMANYAM ET AL.: "contact angle and surface analysis ...", MINERALS ENGINEERING, vol. 9, no. 7, - 1996, gb, pages 727 - 741, XP000987358 * |
Also Published As
Publication number | Publication date |
---|---|
FR2810401B1 (en) | 2002-08-23 |
US20030164027A1 (en) | 2003-09-04 |
EP1301768A1 (en) | 2003-04-16 |
JP2004503741A (en) | 2004-02-05 |
FR2810401A1 (en) | 2001-12-21 |
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